CN116574341B - Graphite composite polystyrene particle and preparation method thereof - Google Patents
Graphite composite polystyrene particle and preparation method thereof Download PDFInfo
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- CN116574341B CN116574341B CN202310850208.1A CN202310850208A CN116574341B CN 116574341 B CN116574341 B CN 116574341B CN 202310850208 A CN202310850208 A CN 202310850208A CN 116574341 B CN116574341 B CN 116574341B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000010439 graphite Substances 0.000 title claims abstract description 55
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 55
- 239000002245 particle Substances 0.000 title claims abstract description 49
- 239000004793 Polystyrene Substances 0.000 title claims abstract description 48
- 229920002223 polystyrene Polymers 0.000 title claims abstract description 48
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims abstract description 44
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical class [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 34
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 22
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000010452 phosphate Substances 0.000 claims abstract description 22
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 22
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 14
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 14
- -1 methyl siloxane Chemical class 0.000 claims abstract description 14
- 239000000375 suspending agent Substances 0.000 claims abstract description 10
- 239000001488 sodium phosphate Substances 0.000 claims abstract description 9
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims abstract description 9
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims abstract description 9
- 235000019801 trisodium phosphate Nutrition 0.000 claims abstract description 9
- 239000003999 initiator Substances 0.000 claims abstract description 8
- 239000004088 foaming agent Substances 0.000 claims abstract description 7
- 239000002667 nucleating agent Substances 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 12
- 239000000376 reactant Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 6
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 6
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 5
- 239000001095 magnesium carbonate Substances 0.000 claims description 5
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- QEQBMZQFDDDTPN-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy benzenecarboperoxoate Chemical compound CC(C)(C)OOOC(=O)C1=CC=CC=C1 QEQBMZQFDDDTPN-UHFFFAOYSA-N 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 12
- 239000003063 flame retardant Substances 0.000 abstract description 12
- 230000000052 comparative effect Effects 0.000 description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- UHGIMQLJWRAPLT-UHFFFAOYSA-N octadecyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCCCCCCCOP(O)(O)=O UHGIMQLJWRAPLT-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 4
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 4
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 4
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 4
- 235000019341 magnesium sulphate Nutrition 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 3
- 239000004795 extruded polystyrene foam Substances 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 229920006248 expandable polystyrene Polymers 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 description 2
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000006261 foam material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920006327 polystyrene foam Polymers 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/08—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing carbon dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/009—Use of pretreated compounding ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/142—Compounds containing oxygen but no halogen atom
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/02—CO2-releasing, e.g. NaHCO3 and citric acid
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/12—Organic compounds only containing carbon, hydrogen and oxygen atoms, e.g. ketone or alcohol
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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- Inorganic Chemistry (AREA)
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Abstract
The invention relates to the technical field of composite materials, and provides graphite composite polystyrene particles and a preparation method thereof, wherein the graphite composite polystyrene particles comprise the following components in parts by weight: 85-95 parts of styrene, 125-135 parts of water, 2-8 parts of graphite, 7-10 parts of foaming agent, 0.1-0.6 part of initiator, 0.08-0.4 part of nucleating agent, 3-8 parts of modified magnesium hydroxide, 0.01-0.05 part of trisodium phosphate, 0.05-0.15 part of inorganic suspending agent, 0.0002-0.0004 part of organic suspending agent and 0.2-0.6 part of polytrifluoropropyl methyl siloxane; the modified magnesium hydroxide is obtained by treating magnesium hydroxide with a treatment solution containing 3-aminopropyl trimethoxy silane and/or stearyl alcohol phosphate. Through the technical scheme, the problem that the flame retardant property and the mechanical property of the graphite composite polystyrene particles in the prior art are poor is solved.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to graphite composite polystyrene particles and a preparation method thereof.
Background
Currently, the external wall heat insulation materials applied in a large scale in the world mainly comprise three types of polyurethane foam, extruded polystyrene foam and expandable polystyrene foam, wherein the expandable polystyrene foam has a plurality of excellent characteristics, such as low heat conductivity coefficient, easy molding and processing, low price and the like, and is widely applied. However, with the widespread use of polystyrene foam materials, their flammable properties are increasingly exposed.
At present, in order to improve the flame retardant effect, a large amount of flame retardant is added into EPS heat insulation materials used in the building industry to improve the flame retardant property, but the stability in the preparation process and the mechanical property of polystyrene particles are reduced due to the large amount of flame retardant, so that development of polystyrene particles with good flame retardant property and mechanical property is needed.
Disclosure of Invention
The invention provides a graphite composite polystyrene particle and a preparation method thereof, which solve the problem of poor flame retardant property and mechanical property of the graphite composite polystyrene particle in the related art.
The technical scheme of the invention is as follows:
the graphite composite polystyrene particles comprise the following components in parts by weight: 85-95 parts of styrene, 125-135 parts of water, 2-8 parts of graphite, 7-10 parts of foaming agent, 0.1-0.6 part of initiator, 0.08-0.4 part of nucleating agent, 3-8 parts of modified magnesium hydroxide, 0.01-0.05 part of trisodium phosphate, 0.05-0.15 part of inorganic suspending agent, 0.0002-0.0004 part of organic suspending agent and 0.2-0.6 part of polytrifluoropropyl methyl siloxane; the modified magnesium hydroxide is obtained by treating magnesium hydroxide with a treatment solution containing 3-aminopropyl trimethoxy silane and/or stearyl alcohol phosphate.
As a further technical scheme, the treatment fluid consists of 3-aminopropyl trimethoxysilane, stearyl alcohol phosphate and water.
As a further technical scheme, the mass ratio of the 3-aminopropyl trimethoxy silane to the stearyl alcohol phosphate in the treatment liquid is 2:0.5-1.5.
As a further technical scheme, the mass ratio of the 3-aminopropyl trimethoxysilane to the stearyl alcohol phosphate in the treatment liquid is 2:1.
According to the invention, when the mass ratio of the aminosilane coupling agent to the stearyl alcohol phosphate in the treatment liquid is 2:1, the prepared graphite composite polystyrene particles have the best compressive strength and flame retardant property.
As a further technical scheme, the sum of the addition amounts of the 3-aminopropyl trimethoxysilane and the stearyl alcohol phosphate is 1-2% of the mass of the treatment fluid.
As a further technical scheme, the preparation method of the modified magnesium hydroxide comprises the following steps: sieving magnesium hydroxide with a 80-mesh sieve, adding into water, stirring, adding 3-aminopropyl trimethoxy silane and stearyl alcohol phosphate, stirring at 80 ℃ for 3 hours, filtering, washing with absolute ethyl alcohol, and drying at 110 ℃ to obtain modified magnesium hydroxide.
As a further technical scheme, the particle size of the graphite is 20-40 mu m.
As a further technical scheme, the foaming agent comprises one or more of magnesium carbonate and isoamyl alcohol.
As a further technical scheme, the initiator comprises one or more of benzoyl peroxide and tert-butyl peroxybenzoate.
The invention also comprises a preparation method of the graphite composite polystyrene particles, which comprises the following steps:
s1, mixing an inorganic suspending agent, an organic suspending agent, trisodium phosphate, graphite, polytrifluoropropyl methyl siloxane and water to obtain a mixture I;
s2, adding an initiator, a nucleating agent, styrene and modified magnesium hydroxide into the mixture I, and mixing and reacting to obtain a reactant I;
s3, adding a foaming agent into the reactant I for reaction to obtain a suspension;
s4, dehydrating, washing and drying the suspension to obtain the graphite composite polystyrene particles.
As a further technical scheme, the reaction in the S2 is carried out at 90 ℃ for 5-7h.
As a further technical scheme, the reaction in the S3 is carried out for 1.5-2.5h at 125-130 ℃.
The working principle and the beneficial effects of the invention are as follows:
1. according to the invention, magnesium hydroxide and graphite are added in the preparation process of the polystyrene particles to improve the flame retardant property of the polystyrene particles, and the addition of the polytrifluoropropyl methyl siloxane improves the dispersion property of the graphite, so that the compressive strength of the graphite composite polystyrene particles is improved, and the flame retardant property is also improved.
2. The magnesium hydroxide added in the invention is modified magnesium hydroxide, and the 3-aminopropyl trimethoxy silane and stearyl alcohol phosphate are used for modifying the magnesium hydroxide together, so that the problem of poor magnesium hydroxide dispersibility is solved, and the flame retardant property of the polystyrene particles is improved while the compressive strength of the graphite composite polystyrene particles is improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the graphite composite polystyrene particles comprises the following steps:
s1, adding 0.05 part of magnesium sulfate, 0.0002 part of hydroxyethyl cellulose, 0.01 part of trisodium phosphate, 2 parts of graphite, 0.2 part of polytrifluoropropyl methyl siloxane and 125 parts of water into a reaction kettle, regulating the rotating speed of the reaction kettle to 350r/min and keeping stable (until a suspension is obtained), and stirring for 30min to obtain a mixture I; wherein the particle size of the graphite is 20 μm;
s2, adding 0.1 part of benzoyl peroxide, 0.08 part of polyethylene wax, 85 parts of styrene and 3 parts of modified magnesium hydroxide into the mixture I, and heating to 90 ℃ for reaction for 5 hours to obtain a reactant I;
s3, adding 7 parts of magnesium carbonate into the reactant I, and reacting for 2.5 hours at the temperature of 125 ℃ to obtain a suspension;
s4, dewatering and washing the suspension, and then placing the suspension into an oven at 80 ℃ to dry for 10 hours to obtain graphite composite polystyrene particles;
the preparation method of the modified magnesium hydroxide comprises the following steps: after passing through a 80-mesh sieve, 10g of magnesium hydroxide is weighed, added into 99g of water, uniformly mixed, added with 0.67g of 3-aminopropyl trimethoxy silane and 0.33g of stearyl alcohol phosphate, stirred for 3 hours at 80 ℃, and subjected to suction filtration, washing with absolute ethyl alcohol and drying at 110 ℃ to obtain the modified magnesium hydroxide.
Example 2
The preparation method of the graphite composite polystyrene particles comprises the following steps:
s1, adding 0.1 part of magnesium sulfate, 0.0003 part of hydroxyethyl cellulose, 0.03 part of trisodium phosphate, 6 parts of graphite, 0.46 part of polytrifluoropropyl methyl siloxane and 130 parts of water into a reaction kettle, regulating the rotating speed of the reaction kettle to 350r/min and keeping stable (until a suspension is obtained), and stirring for 30min to obtain a mixture I; wherein the particle size of the graphite is 30 μm;
s2, adding 0.4 part of benzoyl peroxide, 0.3 part of polyethylene wax, 90 parts of styrene and 6 parts of modified magnesium hydroxide into the mixture I, and heating to 90 ℃ for reaction for 6 hours to obtain a reactant I;
s3, adding 8 parts of magnesium carbonate into the reactant I, and reacting for 2 hours at 128 ℃ to obtain a suspension;
s4, dewatering and washing the suspension, and then placing the suspension into an oven at 80 ℃ to dry for 10 hours to obtain graphite composite polystyrene particles;
the preparation method of the modified magnesium hydroxide comprises the following steps: after passing through a 80-mesh sieve, 10g of magnesium hydroxide is weighed, added into 98.5g of water, mixed uniformly, added with 1g of 3-aminopropyl trimethoxy silane and 0.5g of stearyl alcohol phosphate, stirred for 3 hours at 80 ℃, and subjected to suction filtration, washing with absolute ethyl alcohol and drying at 110 ℃ to obtain the modified magnesium hydroxide.
Example 3
The preparation method of the graphite composite polystyrene particles comprises the following steps:
s1, adding 0.15 part of magnesium sulfate, 0.0004 part of hydroxyethyl cellulose, 0.05 part of trisodium phosphate, 8 parts of graphite, 0.6 part of polytrifluoropropyl methyl siloxane and 135 parts of water into a reaction kettle, regulating the rotating speed of the reaction kettle to 350r/min and keeping stable (until a suspension is obtained), and stirring for 30min to obtain a mixture I; wherein the particle size of the graphite is 40 μm;
s2, adding 0.6 part of tert-butyl peroxybenzoate, 0.4 part of polyethylene wax, 95 parts of styrene and 8 parts of modified magnesium hydroxide into the mixture I, and heating to 90 ℃ for reaction for 7 hours to obtain a reactant I;
s3, adding 10 parts of isoamyl alcohol into the reactant I, and reacting for 1.5 hours at 130 ℃ to obtain a suspension;
s4, dewatering and washing the suspension, and then placing the suspension into an oven at 80 ℃ to dry for 10 hours to obtain graphite composite polystyrene particles;
the preparation method of the modified magnesium hydroxide comprises the following steps: after passing through a 80-mesh sieve, 10g of magnesium hydroxide is weighed, added into 98g of water, mixed uniformly, added with 1.33g of 3-aminopropyl trimethoxy silane and 0.67g of stearyl alcohol phosphate, stirred for 3 hours at 80 ℃, and subjected to suction filtration, washing with absolute ethyl alcohol and drying at 110 ℃ to obtain the modified magnesium hydroxide.
Example 4
Example 4 differs from example 2 in that 1.2g of 3-aminopropyl trimethoxysilane and 0.3g of stearyl alcohol phosphate.
Example 5
Example 5 differs from example 2 in that 0.86g of 3-aminopropyl trimethoxysilane and 0.64g of stearyl alcohol phosphate.
Example 6
Example 6 differs from example 2 in that no stearyl phosphate was added and 1.5g of 3-aminopropyl trimethoxysilane was present.
Example 7
Example 7 differs from example 2 in that no 3-aminopropyl trimethoxysilane was added and the stearyl phosphate was 1.5g.
Comparative example 1
Comparative example 1 differs from example 2 in that 0.5g of 3-aminopropyl trimethoxysilane and 1g of stearyl phosphate.
Comparative example 2
Comparative example 2 differs from example 2 in that 1.3g of 3-aminopropyl trimethoxysilane, 0.2g of stearyl alcohol phosphate.
Comparative example 3
The preparation method of the graphite composite polystyrene particles comprises the following steps:
s1, adding 0.1 part of magnesium sulfate, 0.0003 part of hydroxyethyl cellulose, 0.03 part of trisodium phosphate, 6 parts of graphite, 0.46 part of polytrifluoropropyl methyl siloxane and 130 parts of water into a reaction kettle, regulating the rotating speed of the reaction kettle to 350r/min and keeping stable (until a suspension is obtained), and stirring for 30min to obtain a mixture I; wherein the particle size of the graphite is 30 μm;
s2, adding 0.4 part of initiator, 0.3 part of nucleating agent, 90 parts of styrene and 6 parts of magnesium hydroxide into the mixture I, and heating to 90 ℃ for reaction for 6 hours to obtain a reactant I;
s3, adding 8 parts of magnesium carbonate into the reactant I, and reacting for 2 hours at 128 ℃ to obtain a suspension;
s4, dewatering and washing the suspension, and then placing the suspension into an oven at 80 ℃ to dry for 10 hours to obtain the graphite composite polystyrene particles.
Comparative example 4
Comparative example 4 differs from example 2 in that the polytrifluoropropyl methyl siloxane was not added.
Preparation of polystyrene composite plate:
and adding the graphite composite polystyrene particles prepared in the examples 1-7 and the comparative examples 1-4 into a forming machine according to the mass ratio of the graphite composite polystyrene particles to the curing agent of 100:3, uniformly mixing, and then performing steam heating forming, wherein the pressure of steam is 0.10MPa, and the heating time of introducing steam is 10s, so as to prepare the polystyrene composite board.
The compression strength and oxygen index of the polystyrene composite plates prepared in examples 1 to 7 and comparative examples 1 to 4 were measured as follows:
compressive strength: the compressive strength of the polystyrene composite plate was measured according to the measurement method in GB/T10801.2-2018 extruded polystyrene foam for insulation (XPS);
oxygen index: determination of the Combustion behavior according to GB/T2406.2-2009 Plastic oxygen index method part 2: measuring the oxygen index of the polystyrene composite board by a measuring method in room temperature test;
the measurement results are shown in Table 1.
TABLE 1 results of Performance test of graphite composite polystyrene particles in examples 1 to 7 and comparative examples 1 to 4
Compressive Strength (MPa) | Oxygen index (%) | |
Example 1 | 0.44 | 37.7 |
Example 2 | 0.42 | 38.2 |
Example 3 | 0.35 | 38.5 |
Example 4 | 0.37 | 35.8 |
Example 5 | 0.40 | 37.8 |
Example 6 | 0.25 | 32.4 |
Example 7 | 0.29 | 34.4 |
Comparative example 1 | 0.31 | 36.5 |
Comparative example 2 | 0.34 | 33.8 |
Comparative example 3 | 0.17 | 31.5 |
Comparative example 4 | 0.28 | 30.7 |
In comparison with example 2, example 6 was added with 3-aminopropyl trimethoxysilane alone, example 7 was added with stearyl alcohol phosphate alone, comparative example 3 was not modified with magnesium hydroxide, and as a result, the compressive strength and oxygen index of examples 6 to 7 and comparative example 3 were lower than those of example 2, indicating that the compressive strength and flame retardant properties of the graphite composite polystyrene particles could be improved when magnesium hydroxide was modified with 3-aminopropyl trimethoxysilane and stearyl alcohol phosphate together.
As compared with example 2, comparative examples 1-2 changed the mass ratio of 3-aminopropyl trimethoxysilane to stearyl alcohol phosphate, and as a result, comparative examples 1-2 had lower compressive strength and oxygen index than example 2, indicating that the resulting graphite composite polystyrene particles had higher compressive strength and oxygen index at a mass ratio of 2:1.
Examples 4-5 changed the mass ratio of 3-aminopropyl trimethoxysilane to stearyl phosphate as compared to example 2, and as a result, examples 4-5 had lower compressive strength and oxygen index than example 2, indicating that the compressive strength and oxygen index of the graphite composite polystyrene particles could be further improved when the mass ratio of 3-aminopropyl trimethoxysilane to stearyl phosphate was 2:1.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (8)
1. The graphite composite polystyrene particles are characterized by comprising the following raw materials in parts by weight: 85-95 parts of styrene, 125-135 parts of water, 2-8 parts of graphite, 7-10 parts of foaming agent, 0.1-0.6 part of initiator, 0.08-0.4 part of nucleating agent, 3-8 parts of modified magnesium hydroxide, 0.01-0.05 part of trisodium phosphate, 0.05-0.15 part of inorganic suspending agent, 0.0002-0.0004 part of organic suspending agent and 0.2-0.6 part of polytrifluoropropyl methyl siloxane; the modified magnesium hydroxide is obtained by treating magnesium hydroxide with a treatment solution containing 3-aminopropyl trimethoxy silane and stearyl alcohol phosphate;
the mass ratio of the 3-aminopropyl trimethoxy silane to the stearyl alcohol phosphate in the treatment liquid is 2:1;
the preparation method of the graphite composite polystyrene particles comprises the following steps:
s1, mixing an inorganic suspending agent, an organic suspending agent, trisodium phosphate, graphite, polytrifluoropropyl methyl siloxane and water to obtain a mixture I;
s2, adding an initiator, a nucleating agent, styrene and modified magnesium hydroxide into the mixture I, and mixing and reacting to obtain a reactant I;
s3, adding a foaming agent into the reactant I for reaction to obtain a suspension;
s4, dehydrating, washing and drying the suspension to obtain the graphite composite polystyrene particles.
2. The graphite composite polystyrene particle according to claim 1, wherein said treating fluid is composed of 3-aminopropyl trimethoxysilane, stearyl alcohol phosphate and water.
3. The graphite composite polystyrene particle according to claim 1, wherein the sum of the addition amounts of the 3-aminopropyl trimethoxysilane and the stearyl alcohol phosphate is 1-2% of the mass of the treatment fluid.
4. The graphite composite polystyrene particle according to claim 1, wherein said graphite has a particle size of 20 to 40 μm.
5. The graphite composite polystyrene particle according to claim 1, wherein said foaming agent comprises one or more of magnesium carbonate and isoamyl alcohol.
6. The graphite composite polystyrene particles of claim 1, wherein said initiator comprises one or more of benzoyl peroxide, t-butyl peroxybenzoate.
7. The graphite composite polystyrene particle according to claim 1, wherein said reaction in S2 is carried out at 90 ℃ for 5 to 7 hours.
8. The graphite composite polystyrene particle according to claim 1, wherein said reaction in S3 is carried out at 125-130 ℃ for 1.5-2.5 hours.
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